钟厉,康俊,王振洋,李年,张继祥,韩西.富氧多孔石墨烯薄膜制备及其超级电容器性能[J].表面技术,2024,53(6):198-205.
ZHONG Li,KANG Jun,WANG Zhenyang,LI Nian,ZHANG Jixiang,HAN Xi.Preparation of Oxygen-rich Porous Graphene Film and Performance of Supercapacitor[J].Surface Technology,2024,53(6):198-205 |
| 富氧多孔石墨烯薄膜制备及其超级电容器性能 |
| Preparation of Oxygen-rich Porous Graphene Film and Performance of Supercapacitor |
| 修订日期：2023-04-04 |
| DOI：10.16490/j.cnki.issn.1001-3660.2024.06.018 |
| 中文关键词: 激光诱导技术 多孔石墨烯 氧官能团 超级电容器 |
| 英文关键词:laser-induced technology porous graphene oxygen functional group supercapacitor |
| 基金项目:重庆市自然科学基金面上项目(cstc2020jcyj-msxmX0749);重庆市研究生导师团队建设项目(JDDSTD2019007);重庆市研究生联合培养基地项目(JDLHPYJD2020031);重庆交通大学研究生科研创新项目(CYS22415) |
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| Author | Institution |
| ZHONG Li | School of Mechatronics and Vehicle Engineering,School of Civil Engineering, Chongqing Jiaotong University, Chongqing 400074, China |
| KANG Jun | School of Mechatronics and Vehicle Engineering,School of Civil Engineering, Chongqing Jiaotong University, Chongqing 400074, China |
| WANG Zhenyang | Institute of Solid-State Physics, Hefei Institutes of Physical Science, Chinese Academy of Sciences, Hefei 230031, China |
| LI Nian | Institute of Solid-State Physics, Hefei Institutes of Physical Science, Chinese Academy of Sciences, Hefei 230031, China |
| ZHANG Jixiang | School of Mechatronics and Vehicle Engineering,School of Civil Engineering, Chongqing Jiaotong University, Chongqing 400074, China |
| HAN Xi | School of Mechatronics and Vehicle Engineering,School of Civil Engineering, Chongqing Jiaotong University, Chongqing 400074, China |
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| 中文摘要: |
| 目的 改善传统的激光诱导石墨烯薄膜电极本身储电能力差、应用范围有限的问题。方法 利用CO2激光扫描自制的高含氧酚醛树脂薄膜制备了一种富氧的多孔石墨烯薄膜电极，并对其进行电化学活化处理，用以增强内部含氧基团的活性和含量，对石墨烯薄膜的形貌、组成以及电化学性能进行了表征。结果 在激光的高温高压下，酚醛树脂分解释放的大量气体会使石墨烯薄膜内部形成丰富的纳米孔隙结构，氮气吸附解吸曲线的结果显示其比表面积达到了324 m2/g。此外，在酸性电解质下采用电化学激活的方式，能够使石墨烯薄膜内部碳原子上的含氧基团发生转化反应，并且它们与碳原子的键合也为电极提供了更稳定的结构。在电化学性能测试中，石墨烯薄膜上的氧官能团发生高效的可逆氧化还原反应，在0.5 mA/cm2的电流密度下具有高达342.8 mF/cm2的面积比容量，组装成超级电容器后也保持了优异的储能特性和循环稳定性，在0.058 9 mW/cm2的功率密度下具有5.93 μWh/cm2的能量密度。结论 利用该方法制备的富氧多孔石墨烯电极材料兼具高稳定性和高比电容的优势，有望在实际应用中为后续赝电容材料的可靠负载和异原子的高含量稳定掺杂提供一种更可靠的石墨烯骨架，为构筑新型高性能储能器件提供了设计思路。 |
| 英文摘要: |
| Graphene material is one of the most reliable electrodes for supercapacitors, which shows outstanding characteristics, such as high crystal quality, 3D net-work and large specific surface area. Among numerous methods of preparing graphene, laser-induced technology can select different carbon precursors to prepare graphene with different properties, which displays differences in electrochemical performance. Therefore, an oxygen-enriched porous graphene electrode was prepared through CO2 laser scanning by the self-made phenolic resin film with high oxygen content, which effectively improved the limited energy storage capacity of traditional laser-induced pure graphene film electrode materials and its application prospect. 6 g of phenolic resin (PR) powder and 17.5 mL of anhydrous ethanol were evenly mixed to obtain 20 mL of PR solution. Part of the ethanol was evaporated at 85 ℃ until the solution was 15 mL and the PR solution changed to PR colloid, which presented excellent film forming ability and rich oxygen content. The prepared PR colloid was made into 100 μm film on PET substrate by wire applicator. Then, the oxygen-enriched carbon precursor was scanned into graphene material by HanS CO2-D200 laser device, and the corresponding laser parameters were below:(i) laser power of 5 W; (ii) laser scanning line spacing of 0.15 mm; (iii) laser scanning speed of 30 mm/s. In addition to its own advantages, the graphene prepared under this condition also had the characteristics of oxygen enrichment. Therefore, electrochemical activation at the voltage sweep rate of 10 mV/s was selected to treat the oxygen-rich porous graphene material film. Then, the microstructure of graphene film was characterized by Gemini SEM 500 scanning electron microscope and JEM-2100 F transmission electron microscope. Apart from the morphology, the phase of graphene film was analyzed by X-ray diffractometer (X-ray diffraction of Cu Kα radiation). Raman spectra was captured by DXR Raman microscope under 532 nm laser excitation. Fourier transform infrared spectrum was captured by FT-IR spectrometer (MagnaIR 750) to explore the changes of oxygen-containing groups in graphene film before and after activation. Contact angle meter (JC2000D1, CA-D type) was used to measure the wettability before and after activation. The specific surface area of graphene film was measured by TriStarII3020M. Finally, the electrochemical workstation of CHI760E was used to analyze the properties of graphene film and assembled device. It is found that under high temperature and pressure of laser beam, a plenty of gas is released by the decomposition of phenolic resin, which will promote the formation of abundant nanopore structure inside the graphene film material. The results of nitrogen adsorption-desorption indicate that the specific surface area of the prepared graphene film reaches 324 m2/g. In addition, the transformation of the oxygen functional groups in graphene can be achieved by electrochemical activation under acidic electrolytes, and their bonding with carbon atoms also provides a more stable structure for the electrode. In the electrochemical performance test, the oxygen-containing groups provide an efficient reversible redox reaction, and deliver an area specific capacity of up to 342.8 mF/cm2 at the current density of 0.5 mA/cm2, and still retain the high value of 192 mF/cm2 at 3 mA/cm2. Compared with the graphene film not activated (12.6 mF/cm2 at 3 mA/cm2), the capacitance increases by nearly 15 times. After being assembled into a supercapacitor, it also maintains excellent energy storage characteristics and cycle stability, which demonstrates an energy density of 5.93 μWh/cm2 at a power density of 0.058 9 mW/cm2. Oxygen-rich porous graphene thin film electrode material is prepared by simple and controllable laser induction technique and electrochemical activation treatment in this work, which demonstrates its advantages of high stability and excellent specific capacitance, providing a new design for the preparation of energy storage device. |
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